Method of and apparatus for extracting constituents of mineral oils



Jan. 24, 1939. 2,144,797

METHOD oF AND APPARATUS FOR ExTRAcTING coNsTITURNTs oF MINERAL OILS E. M. DONS` ET AL Filed July 1l 2 Sheets-Sheet lv .SOL T/oN .1911.24, 1939. E. M. DONS n AL f 2,144,797

METHODKOF AND APPARATUS FOR EXTRACTING CONSTITUENTS OF MINERAL OILS I Filed July ll, 1936 2 Sheets-Sheet 2 Patented Jan. 24, 1939 MErnoD oF AND APPARATUS Foa nx- 'rnAo'rlNG ooNs'rnUEN'rs or MINERAL GILS Eddie M. Dons, omis G. Mauro, ma Dwight n.

Tulsa, Okla., assignors to Mid-Continent Petroleum Corporation,` Tulsa, Okla., a' corporation of Delaware Application July 11,

6 Claims.

'I'his invention relater to methods of and apparatus for extracting constituents of mineral oils. The invention-may be used with selective solvents for the separation of naphthenic and paramnic constituents of mineral oils, especially kin the manufacture of petroleum lubricating oils having high viscosity indexes.

An object of the invention is to very effectively separate lthe dierent constituents of 'the oils.

lTo illustrate this .feature we will hereafter describe a system wherein kcounterilowing solutions of the oil and solvent are divided into numerous relatively thin layers which flow radially in opposite directions, to provide a very large total l5 area at the contactingfaces'of the different layers, thereby providing a high degree of efficiency in the transfer of selected constituents from each layer to the oppositely moving layer contacting therewith. In addition to forming the numerous relatively thin counterfiowing layers, we have produced a condition wherein there isv frequent mixing of the layers while they moveinintersecting paths at relatively high speeds, followed by correspondingly frequent settling at `lower al speeds, all of which results in avery effective transfer of the selected constituents from one layer to another. Y

With the foregoing and other objects in view, the invention comprises the novel method, conao struction, combination and arrangement of parts hereinafter more specically described and shown in the accompanying drawings, which illustrate one form of the invention. However, it is to be understood that the invention comprehends as changes, variations and modiiications within the scope of the claims hereunto appended.

Fig. 1 is a diagrammatical view of a'system embodying features of this invention.

Fig. 2 is a fragmentary section on a larger 40 scale, with arrows diagrammatically indicating` thepaths of counterflowing solutions in the extracting column. r Fig. 3 is a horizontal section on theline 3 3 in Fig. 2, indicating the radial flow which results in a relatively high speed at a mixing zone near the centerof the column, and lower speeds in a' settling zone aroundsaid mixingzone.

Fig. 4 is a vertical section of the upper portion of the extracting column. 50 Fig. 5 is a similar view of the lower portion of said extracting column.

To illustrate one form of the invention we have shown an extracting chamber in the form of a tall column A, having'an upper portion (Figures Il l and 4) provided with an inlet pipe I for a se- 1936, ASel'lal No. 90,064

(Cl. 11W-13) lective extracting solvent, and a discharge pipe 1 leading to a storage tank 8 for the parafnic solution. 'I'he supply of fresh solvent is constantly discharged from a tank 8 (Fig. 1) to a pump I0 which forces the fresh solvent through a heatexchanger il tothe inlet pipe 6. The heat-ex# changer Il may be used to either heat or cool theincoming solvent, depending upon the operating conditions.

The lower portion of the extracting'column A (Figures 1 and 5) is provided with an inletpipe I2 for'oil to be extracted, and a discharge pipe i3 for naphthenic solution which gradually settles to the bottom of the extracting column. Instead of immediately discharging this naphthenic `solution from the system, it cany be conveniently employed for an initial extraction of the incoming oil. For example, the oil stock to be treated may; be constantly discharged from a tank Il (Fig. 1) through a pipe I5 and pump i6 leading to' a heat-exchanger Il which discharges through a pipe il leading to a mixer i9 and thence to an initial extracting chamber, or settling chamber 2li. The naphthenic solution from the bottom of the extracting column A may be conducted through pipe II' to the pipe i8, where it enters into the constant stream of fresh oil passing to the mixer I9. r This mixture of fresh oil and degradednaphthenic solution is permitted to settle and separate in the initial extracting chamber 20, where the relatively parafllnic oil solution to be hereafter mentioned, is constantly discharged at the top through a pipe 2|, while the naphthenic solution Vis constantly discharged at the bottom through a pipe 22. 4s a further step to recover valuable f paraillnic material from' the naphthenic solution discharged through pipe 22, saidpipe may be connected to an intermediate extracting chamber 23 where the degraded naphthenic solution is constantly discharged at the bottom and conducted through pipe 24 toa storage tank 25.

The paraillnic solution rising to the top of the intermediate extracting chamber 23 is discharged through a pipe 20 tothe pipe 2| where it merges into the stream of solution from the initial extracting chamber 20. 'Ihe resultant solution comprising portions of the solvent united with oil stock that has been subjected to preliminary extractions,A is transmitted through a mixer 2l' to the inlet pipe I2 leading into the lower portion of the extractingrcolumn A.

The naphthenic solution discharged through pipe Il at the bottom of the extracting column A. can be thusutilized for preliminary extractions of the incoming oil before it reaches the inlet pipe l2 of the main extracting column A, one of the objects being to use this naphthenlc solution for relatively simple preliminary extractions, in advance of the more difdcult subsequent extracting operations to' be performed in the column A.

The oil solution entering through pipe I2 at the lower portion of the column A (Figures 1 and 5) merges ,into the heavy naphthenlc solution at this point. The light paraiilnic constituents gradually rise through this column until they are eventually discharged at the top through the pipe 1 leading to the tank 8 for storage of the paraiiinic solution. Heavy naphthenlc constituents are gradually extracted and eventually flow to the bottom of the column, where they are discharged through the pipe i8.

Attention is now directed to the interior of the extracting column A where the light and heavy y inner face of the column, and an approximatelyv central opening 88 through which the diilerent solutions vrise and fall inpassing from one of the baille plates to another. Y

By referring to Figures 2, 3 and 4 it will be understood that the solutions of oil and solvent are divided into numerous thin layers of different specific gravities contacting with each other. These contacting layers move radially in opposite directions, and at gradually changing speeds. toward and away from the central portion of the column. The highest speed is attained near the centralportion of 'the column where al1 of the liquid must pass through a relatively small opening l0, while the lowest speed is near the periphery where approximately the same volume of liquid ilows through a much larger opening between the periphery of a baille plate 28 and the inner face of the' column.

Mixing zones are formed at the central openings 88 where the oppositely moving layers travel in intersecting paths from one plane to another at-a'relatively high speed. The resultant mixtures are permitted to settle and stratify at lower speeds around the central mixing zone, the speed of each layer being gradually increased as it moves toward the central mixing zone and gradually decreased as it moves away from said mixing zone. The oppositely moving layers also travel through intersecting paths-in the zones of lowest speed around the peripheries of the baille plates 28, so as to provide secondary mixing zonesV alternating with the primary mixing zones at the central portion of the column. v v The fresh solvent which enters at the upper portion of the column is thus combined with oil that enters at the lower portion of thecolumn to provide numerous relatively thin layers distrib- .'uted throughout the column in such manner that the natural counterow is frequently interrupted by mixing at relatively high speeds and settling at lower speeds. The surface contact is very greatly increased, and the selective action of the solvent is effectively obtained in merely transferring constituents of one thin layer to another thin layer. central mixing zones is not violent enough to form an objectionable emulsion, but sumcient to Furthermore, the agitation at ther the center of the column to a zone of lowest speed at the periphery of the column has a further advantage in heating or cooling all \of the numerous streams in the low speed zo\nes at the periphery. The heat transfer is most effective at the periphery of the column where there is a large area of surface contact between substantially all of the constituents of the different solutions and the inner face of the column. A jacket surrounding this column could be most effectively utilized to heat or cool the streams bf liquid in vthe column.

The column herein shown is composed of six iianges 82 atthe topand bottom of the section. To provide for the transfer of any desired heatexchangers 33 (Fig. 1). The heatlngor-cooling iluid may flow in the directions indicated by arrows in Figures ,1, 4 and 5, or the flow may be reversed, depending upon the temperatures desired in the column, and the .temperature of the incoming fluid. 'For example, if a cool fluid is introduced near the bottom to provide successive increases in temperatureI toward the top, the heatexchangers 38 are employed to gradually increase the temperature of the cool fluid. This will progressively increase the temperature of the internal layers as theypass from the naphthenlc phases inthe lower portion of the column to the parailinic phasesin the upper portion of said column, and the heat transfer will occur around is at a temperature of 10 F. to 30 F. lower than.

the top. v

A .further advantage can be gained by so arranging the baille plates 28 and 28 that the disling or cooling iluid from one jacket to another, I

said jackets are connected by means of heattance between said plates is .progressively decreased toward the upper portion of the column.

This is shown in Figures 4 and 5. It progressively decreases the thickness of the layers as they pass from relatively naphthenicphases in the phases in the upper portion of said column. This variation in the thicknesses of the different layers results in a more effective selective action of the solutions at the several elevations where .the conditions as to ratios of solvent and parafilnic and naphthenlc constituents are undergoing constant changes. For example, in a desirable form of the invention, most of the selective solvent passes out with naphthenlc compounds at the bottom of thev column, and a very eifective selective action can be obtained by producing relatively thin layers at the top, where the fresh solvent enters into more valuableportions of the mixture, to be discharged as the paralnic solution, containing a veryy small percentage of the solvent. The paramnic solution discharged at the top may be .lower portion of the column tol more lparaiiinic lo parts, compared with 13o-parts in the naphthenic solution discharged at the bottom, but this,`

advantages of preliminary or subsequent extrac-` tions, we treated a petroleum lubricating oil stock having an A, P. I. gravityfof 25.8, a Saybolt Universal viscosity oi 251 at100 F. and 48.2 at

210 F. The selective solvent was beta beta prime dichlorethyl ether, and we used 1.8 parts of this solvent to l part of the original oil. The resultant parailinic oil, after the solvent was distilled there-` from, had an A. P. I. gravity of 29.9, and a viscosity index of 102.6. 'I'he yield of this valuable that the temperatures and proportions of the oil j and solvent may be varied as desired. Examples of such solvents are dischlorethyl ether, cresylic acid, iuriural, and nitrobenzene. It will also be understood that the solvents can be recovered Y from the paramnic and naphthenic solutions by distillation, or in any other suitable manner.

-We claim:

1. In the art of using selective solvents to separate paraiilnic and naphthenic constituents oi mineral oils, the method which comprises 'transcausing said layers to move radially in op- -f posite directions toward and away from the central portion of said chamber, and at gradually changing speeds, the highest speed being near vsaid central portion and the lowest being near the periphery of said chamber, causing said oppositely moving layers to advance in intersecting paths while ilowing from one plane to another at the central zones of relatively high-speed, thereby mixing vconstituents oi.' the diilerent layers, as they advance at saidrelatively high speed, permitting the mixtures to settle and stratify at lower speeds around the central mixing zone, causing the oppositely moving layers to progress through the numerous mixing and settling zones, and separately discharging the light and heavy liquids from said chamber.

2. In the art oi using selective solvents -to separate paraillnic and naphthenic constituents of mineral oils, the method which comprises transmitting mineral oil and the selective solvent into a separating chamber, dividing the resultant solutions into layers of dinerent specific gravlties contacting with each other-,causing said'layers to move radially in opposite directions and at gradually changing speeds toward and away from the central portion of said chamber, the highest speed being near said central portioniand the lowest being'near the periphery of said chamber,

o causing said oppositely moving layers to advance zone and gradually decreasedl as it moves away from said mixing zone, causing the oppositely moving layers to progress through the mixing and settling zones, and separately discharging the paraillnic and naphthenic solutions rom said chamber. l

'3. In the art of using selective solvents to separate paraiilnic and naphthenic constituents oi lubricating oils, the method which comprises ytransmitting the lubricating oil stock and the selective solventinto an upright separating column, dividing the resultant solutions into numerous-thin, approximately horizontal layers of dif- -ferent specific gravlties. contacting vwith each other, causing said approximately horizontal layers to move radially in opposite directions and at gradually changing speeds toward and away from the central-portion of said column, the highest speedbeing near said central portion and the lowest being near the periphery of said column, causing said oppositely` 'moving layers to ilow in intersecting paths from one plane to another atv the central zones of relatively high speed, thereby mixing constituents of the different layers, permitting the mixtures to settle and stratify at lower speeds in approximately horizontal planes around the central mixing zone, the speed of each layer being gradually increased as it moves tolward the central mixing zone and gradually decreased as it movesaway from said mixing zone, causing the oppositely moving layers to progress through the numerous mixing and settling zones, and separately discharging the paraiiinic and naphthenic solutions from said column.

4. In the art of using selective solvents to sepa.- rate paramnic and naphthenic constituents of `mineral oils, the method which comprises transmitting mineral oil and the selective solvent into an upright separating column, dividing the resultant solutions into approximately horizontal layers of different speciiic gravlties contacting with each other, 'causing said approximately hori- .v zontal layers to move radially in opposite direc- -tions toward and away from the central portion oi said column, and at gradually changing speeds, the highest speed being near said central portion and the lowest being near the periphery of said column, causing said oppositely moving layers to advance in intersecting paths while flowing from one plane to another at the central zones of relatively high speed, thereby mixing constituents of the diierent layers, permitting the mixtures to settle and stratify at lower speeds around the central mixing zone, causing the oppositely moving layers to progress through the several miidng and settling zones, progressively decreasing the thickness of said layers as they pass from relatively naphthenic phases in the lower portion oi' said column to more paranic phases in the upper portion of said column, and separately discharging the paraninic and naphthenic solutions from said column.

5. In the art of using selective solvents to separate paraiiinic and naphthenic constituents of mineral oils, the method which comprises transmitting mineral oil and the selective solvent into an upright separating chamber, dividing the resultant solutions into numerous thin, approximately horizontal layers oi different specic gravities contacting with each other, causing said layers to move radially in opposite directions toward andV away from the central portion .of said chamber, and at gradually changing speeds, the highest speed being near said central portion and the lowest being near the periphery of said chamber, causing said oppositely moving layers to advance in intersecting paths While flowing from one plane to another at the central zones of relatively high speed, thereby mixing constituents of the different layers, permitting the mixtures to settle and stratify at lower speeds around the central mixing zone, causing the oppositely moving layers to progress through the numerous mixing and settling zones, progressively increasing the temperature of said layers as they pass from the naphthenic phases in the lower portion of said chamber to the parailinic phases in the upper portion of said chamber, and separately discharging the paraflinic and naphthenic solutions from said chamber.

S. In an apparatus for separating paramnic and naphthenic constituents of mineral oils, an extracting column having an upper portion provided with an inlet for an extracting solvent and an outlet for paratlinic solution, a lower portion of said column being provided with an inlet for oil to be extracted and an outlet for naphthenic solution, and a series of baffles in said column, said baiiles comprising plates having peripheral edges separated from the inner face of the column alternating with plates having peripheral portions united with the inner face of the column, the last mentioned plates being provided with approximately central openings through which the different solutions rise and fall in passing from one of said plates to another', the distance between said alternating plates being progressively decreased toward the upper portion of the column.

- EDDIE M. DONS.

OSWALD G. MAURO. DWIGHT B. MAPES. 

